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Fluidized-bed pyrolysis reactor produces high-purity polycrystalline silicon from silane or halosilane via efficient heterogeneous deposition of silicon on silicon seed particles. Formation of silicon dust via homogeneous decomposition of silane minimized, and deposition of silicon on wall of reactor effectively eliminated. Silicon used to construct solar cells and other semiconductor products.
Fluidized-bed reactor produces highly pure polycrystalline silicon particles with diameters approximately greater than 400 micrometers. Operates by pyrolysis of silane in reaction zone, which is bed of silicon seed particles fluidized by flow of silane and carrier gas. Above reaction zone, gas mixture flows rapidly enough to entrain silicon powders, but not larger seed and product particles. Entrained particles swept out of reactor. Applicable to other processes such as production of fine metal and ceramic powders where control of sizes of product needed.
This report summarizes a three-year collaborative effort between researchers at UMPQUA Research Company (URC) and the Chemical Engineering Department at Oregon State University (OSU). The Magnetically Assisted Gasification (MAG) concept was originally conceived as a microgravity and hypogravity compatible means for the decomposition of solid waste materials generated aboard spacecraft, lunar and planetary habitations, and for the recovery of potentially valuable resources. While a number of methods such as supercritical water oxidation (SCW0), fluidized bed incineration, pyrolysis , composting and related biological processes have been demonstrated for the decomposition of solid wastes, none of these methods are particularly well- suited for employment under microgravity or hypogravity conditions. For example, fluidized bed incineration relies upon a balance between drag forces which the flowing gas stream exerts upon the fluidization particles and the opposing force of gravity. In the absence of gravity, conventional fluidization cannot take place. Hypogravity operation can also be problematic for conventional fluidized bed reactors, because the various factors which govern fluidization phenomena do not all scale linearly with gravity. For this reason it may be difficult to design and test fluidized bed reactors in lg, which are intended to operate under different gravitational conditions. However, fluidization can be achieved in microgravity (and hypogravity) if a suitable replacement force to counteract the forces between fluid and particles can be found. Possible alternatives include: centripetal force, electric fields, or magnetic fields. Of these, magnetic forces created by the action of magnetic fields and magnetic field gradients upon ferromagnetic media offer the most practical approach. The goal of this URC-OSU collaborative effort was to develop magnetic hardware and methods to control the degree of fluidization (or conversely consolidation) of granular ferromagnetic media and to employ these innovations in sequential filtration and fluidized bed processes for the segregation and decomposition of solid waste materials, and for the concentration and collection of inorganic residue (ash). This required the development of numerous enabling technologies and tools.
A process and apparatus for thermally decomposing silicon containing gas for deposition on fluidized nucleating silicon seed particles is disclosed. Silicon seed particles are produced in a secondary fluidized reactor by thermal decomposition of a silicon containing gas. The thermally produced silicon seed particles are then introduced into a primary fluidized bed reactor to form a fluidized bed. Silicon containing gas is introduced into the primary reactor where it is thermally decomposed and deposited on the fluidized silicon seed particles. Silicon seed particles having the desired amount of thermally decomposed silicon product thereon are removed from the primary fluidized reactor as ultra pure silicon product. An apparatus for carrying out this process is also disclosed.
A continuing program of research and development has been directed toward improvement of a prior batch process in which single-walled carbon nanotubes are formed by catalytic disproportionation of carbon monoxide in a fluidized-bed reactor. The overall effect of the improvements has been to make progress toward converting the process from a batch mode to a continuous mode and to scaling of production to larger quantities. Efforts have also been made to optimize associated purification and dispersion post processes to make them effective at large scales and to investigate means of incorporating the purified products into composite materials. The ultimate purpose of the program is to enable the production of high-quality single-walled carbon nanotubes in quantities large enough and at costs low enough to foster the further development of practical applications. The fluidized bed used in this process contains mixed-metal catalyst particles. The choice of the catalyst and the operating conditions is such that the yield of single-walled carbon nanotubes, relative to all forms of carbon (including carbon fibers, multi-walled carbon nanotubes, and graphite) produced in the disproportionation reaction is more than 90 weight percent. After the reaction, the nanotubes are dispersed in various solvents in preparation for end use, which typically involves blending into a plastic, ceramic, or other matrix to form a composite material. Notwithstanding the batch nature of the unmodified prior fluidized-bed process, the fluidized-bed reactor operates in a continuous mode during the process. The operation is almost entirely automated, utilizing mass flow controllers, a control computer running software specific to the process, and other equipment. Moreover, an important inherent advantage of fluidized- bed reactors in general is that solid particles can be added to and removed from fluidized beds during operation. For these reasons, the process and equipment were amenable to modification for conversion from batch to continuous production.
To support long-duration manned missions in space such as a permanent lunar base, Mars transit, or Mars Surface Mission, improved methods for the treatment of solid wastes, particularly methods that recover valuable resources, are needed. The ability to operate under microgravity and hypogravity conditions is essential to meet this objective. The utilization of magnetic forces to manipulate granular magnetic media has provided the means to treat solid wastes under variable gravity conditions by filtration using a consolidated magnetic media bed followed by thermal processing of the solid wastes in a fluidized bed reactor. Non-uniform magnetic fields will produce a magnetic field gradient in a bed of magnetically susceptible media toward the distributor plate of a fluidized bed reactor. A correctly oriented magnetic field gradient will generate a downward direct force on magnetic media that can substitute for gravitational force in microgravity, or which may augment low levels of gravity, such as on the Moon or Mars. This approach is termed Gradient Magnetically Assisted Fluidization (G-MAFB), in which the magnitude of the force on the fluidized media depends upon the intensity of the magnetic field (H), the intensity of the field gradient (dH/dz), and the magnetic susceptibility of the media. Fluidized beds based on the G-MAFB process can operate in any gravitational environment by tuning the magnetic field appropriately. Magnetic materials and methods have been developed that enable G-MAFB operation under variable gravity conditions.
A Process Development Unit (PDU), which consisted of the four major units of the process, was designed, installed, and experimentally operated. The PDU was sized to 50MT/Yr. The deposition took place in a fluidized bed reactor. As a consequences of the experiments, improvements in the design an operation of these units were undertaken and their experimental limitations were partially established. A parallel program of experimental work demonstrated that Zinc can be vaporized for introduction into the fluidized bed reactor, by direct induction-coupled r.f. energy. Residual zinc in the product can be removed by heat treatment below the melting point of silicon. Current efficiencies of 94 percent and above, and power efficiencies around 40 percent are achievable in the laboratory-scale electrolysis of ZnCl2.
Laboratory scale experiments were conducted on two high volatile bituminous coals in a bench scale batch fluidized bed reactor. Chemical pretreatment and posttreatment of coals were tried as a means of enhancing desulfurization. Sequential chlorination and dechlorination cum hydrodesulfurization under modest conditions relative to the water slurry process were found to result in substantial sulfur reductions of about 80%. Sulfur forms as well as proximate and ultimate analyses of the processed coals are included. These studies indicate that a fluidized bed reactor process has considerable potential for being developed into a simple and economic process for coal desulfurization.
The production process of solar grade silicon (SOG-Si) through trichlorosilane (TCS) was researched in a program sponsored by New Energy Development Organization (NEDO). The NEDO process consists of the following two steps: TCS production from by-product silicon tetrachloride (STC) and SOG-Si formation from TCS using a fluidized bed reactor. Based on the data obtained during the research program, the manufacturing cost of the NEDO process and other polysilicon manufacturing processes were compared. The manufacturing cost was calculated on the basis of 1000 tons/year production. The cost estimate showed that the cost of producing silicon by all of the new processes is less than the cost by the conventional Siemens process. Using a new process, the cost of producing semiconductor grade silicon was found to be virtually the same with any to the TCS, diclorosilane, and monosilane processes when by-products were recycled. The SOG-Si manufacturing processes using the fluidized bed reactor, which needs further development, shows a greater probablility of cost reduction than the filament processes.
In order for efficient multimegawatt closed cycle nuclear-MHD systems to become practical, long-life gas cooled reactors with exit temperatures of about 2500 K or higher must be developed. Four types of nuclear reactors which have the potential of achieving this goal are the NERVA-type solid core reactor, the colloid core (rotating fluidized bed) reactor, the 'light bulb' gas core reactor, and the 'coaxial flow' gas core reactor. Research programs aimed at developing these reactors have progressed rapidly in recent years so that prototype power reactors could be operating by 1980. Three types of power plant systems which use these reactors have been analyzed to determine the operating characteristics, critical parameters and performance of these power plants. Overall thermal efficiencies as high as 80% are projected, using an MHD turbine-compressor cycle with steam bottoming, and slightly lower efficiencies are projected for an MHD motor-compressor cycle.
Mars Design Reference Architecture 5.0:Lists in-situ resource utilization (ISRU) as enabling for robust human Mars missionsLO2LCH4 ascent propulsion 25,000 kg oxygen from atmosphere for ascent and life support Atmospheric based ISRU processes less operationally complex than surface based limited concept evaluation to date and Mars surface water property and distribution uncertainty would not allow [Mars soil water processing] to be base lined at this time Limited Concept Evaluation to Date Lunar regolith O2 extraction processing experience Lunar regolith is fluidized and heated to high temperatures with H2 to produce H2O from iron-bearing minerals Mars similarity concept: Soil placed in fluidized bed reactor Heated to moderate temperatures Inert gas flow used to fluidize the bed and help with water desorption Challenges: High-temperature dusty seals Working gas requires downstream separation and recycling to reduce consumables loss Batch process heating thermally inefficient.
A report presents a numerical-simulation study of pyrolysis of biomass in fluidized-bed reactors, performed by use of the mathematical model described in Model of Fluidized Bed Containing Reacting Solids and Gases (NPO-30163), which appears elsewhere in this issue of NASA Tech Briefs. The purpose of the study was to investigate the effect of various operating conditions on the efficiency of production of condensable tar from biomass. The numerical results indicate that for a fixed particle size, the fluidizing-gas temperature is the foremost parameter that affects the tar yield. For the range of fluidizing-gas temperatures investigated, and under the assumption that the pyrolysis rate exceeds the feed rate, the optimum steady-state tar collection was found to occur at 750 K. In cases in which the assumption was not valid, the optimum temperature for tar collection was found to be only slightly higher. Scaling up of the reactor was found to exert a small negative effect on tar collection at the optimal operating temperature. It is also found that slightly better scaling is obtained by use of shallower fluidized beds with greater fluidization velocities.
Experimental coal-desulfurization process uses alkalies and steam in fluidized-bed reactor. With highly volatile, high-sulfur bituminous coal, process removed 98 percent of pyritic sulfur and 47 percent of organic sulfur. Used in coal liquefaction and in production of clean solid fuels and synthetic liquid fuels. Nitrogen or steam flows through bed of coal in reactor. Alkalies react with sulfur, removing it from coal. Nitrogen flow fluidizes bed while heating or cooling; steam is fluidizing medium during reaction.
Correct placement helps prevent contamination while eliminating crack-causing deposits. Repositioning quartz liner in silicon fluidized-bed reactor prevents cracking of liner when cools. Liner protects stainless-steel walls of reactor from abrasion by particles in fluidized bed. Prevents contamination of newly formed silicon by material abraded from wall and ensures high-quality product.
A process and apparatus for thermally decomposing silicon containing gas for deposition on fluidized nucleating silicon seed particles is disclosed. Silicon seed particles are produced in a secondary fluidized reactor by thermal decomposition of a silicon containing gas. The thermally produced silicon seed particles are then introduced into a primary fluidized bed reactor to form a fludized bed. Silicon containing gas is introduced into the primary reactor where it is thermally decomposed and deposited on the fluidized silicon seed particles. Silicon seed particles having the desired amount of thermally decomposed silicon product thereon are removed from the primary fluidized reactor as ultra pure silicon product. An apparatus for carrying out this process is also disclosed.
A report presents an assessment of a general mathematical model of dense, chemically reacting granular flows like those in fluidized beds used to pyrolize biomass. The model incorporates submodels that have been described in several NASA Tech Briefs articles, including "Generalized Mathematical Model of Pyrolysis of Biomass" (NPO-20068) NASA Tech Briefs, Vol. 22, No. 2 (February 1998), page 60; "Model of Pyrolysis of Biomass in a Fluidized-Bed Reactor" (NPO-20708), NASA Tech Briefs, Vol. 25, No. 6 (June 2001), page 59; and "Model of Fluidized Bed Containing Reacting Solids and Gases" (NPO- 30163), which appears elsewhere in this issue. The model was used to perform computational simulations in a test case of pyrolysis in a reactor containing sand and biomass (i.e., plant material) particles through which passes a flow of hot nitrogen. The boundary conditions and other parameters were selected for the test case to enable assessment of the validity of some assumptions incorporated into submodels of granular stresses, granular thermal conductivity, and heating of particles. The results of the simulation are interpreted as partly affirming the assumptions in some respects and indicating the need for refinements of the assumptions and the affected submodels in other respects.
Silicon deposition on silicon seed particles by silane pyrolysis in a fluidized-bed reactor is investigated as a low-cost, high-throughput method to produce high-purity polysilicon for solar-cell applications. Studies of fines, particles 0.1-10 microns diam, initiated from homogeneous decomposition in the reactor were conducted using 2 and 6-in-diam fluidized beds. The studies show functional dependences of fines elutriation on silane feed concentration, temperature, gas velocity, and bubble size. The observation that the fines elutriation is generally below 10 percent of the silicon-in-silane feed is attributed to scavenging by large particles in an environment of less free space for homogeneous nucleation. Preliminary results suggest that, with proper conditions and distributor design, high-silane-concentration (over 50 percent SiH4 in H2) feed may be used.
The model is intended for use as a means of improving fluidized bed reactor design and for the formulation of the research program in support of the contracts of Silicon Material Task for the development of the fluidized bed silicon deposition process. A computer program derived from the simple modeling is also described. Results of some sample calculations using the computer program are shown.